Recovery of tar and ammonia from coal-gas.



G. STILL.

RECOVERY OF TAB AND AMMONIA FROM (EOAL GAS.

APPLICATION FILED no.3. 1912.

1,08%988, Patented Dec. 9, 1913.

' CAR-L STILL, or nnexnrnonnnsnn, GERMANY.

RECOVERY OF TAB AND AMMQNIA FROM QUAIL-GAS.

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To all whom it may concern:

Be it known that I, Can STILL, a .sub e ct of the German Emperor, residing at Basmarekplatz, ltecklinghausen, Germany, have.-

invented certain new and useful Improvementsin the Recovery of Tar and Anamonia from Coal-Gas, of which the follow.- ing is a specification.

My invention relates .to a method of separating tar and ammoniafrom gases obtained by the dry distillation .or gasification of the coal, and aims atthe recovery of these two by-products in a manner very profitable and avoiding all faults of ,the methods"heretofore known.

The method, hereinafter described, is based upon the idea to cool down first the hot crude ases to about atmospheric temperature hereby, the tar is completely removed, and then to heat afterward thegases freed from tar to such a temperature gthat they absorb'again in form of steam the water condensed through the previous cooling, So that finally the gases contain the whole quantity of water, and hence also the Whole quantity of ammonia originally contained in the crude gases but no traces of tar, and can be subjected in this state to the process of ammonia absorption by means of acid.

The cooling :as well as the'subsequent reheating of the gases is made directly by means of water injected or otherwise brought into intimate contact with the igases by any suitable means in such a way .t iat a certain quantity of water is used alternately first for the cooling during which process it ab sorbs heat and is increased at the same time by the volume of the water condensed out of the cooled gases, and that afterward the water heated .in the first stage is used for the direct reheating of the cooled gases whereby, on the one hand, the water is again cooled on the other hand, the quantity of the water condensed duringthe cooling of the gases is rendered again to the gases in form of steam. It results therefrom that a continuous circulation of the said quantity of water takes place, the gases as well as the water being continuously cooled and reheated.

The drawing annexed shows, partlyin a vertical section, partly as a direct view an arrangement which can be used for the working of the process.

Specification of Letters Patent.

Patented Dec. 9, 1913.

Application filed December 3, 1912. Serial No. 734,708.

The method of working isa's follows The letter A designates the apparatus used for directly cooling the hot gases, B the apparatus serving the direct heating of the gases, and .C an intermediate cooler acting indirectly. The tanks E and F serve the storage of the liquids flowing from the apparatus A- and B. The saturater marked 1) is .used for the absorption of the ammonia from the gases, and K is a cooler for finally cooling the completely treated gases. The gas to be treated enters in a hot state the cooler A-arranged for direct cooling-at aiby theaction (of theexhauster G, and rises upward, encountering a stream of -WLfif serving as a cooling medium. The Water is taken out .Of'.th6 ftank F by means of the pump H, injected into the vcooler A at its top part by means of the distribution nozzles c and brought into intimate contact with the gases by a series of perforated sheets '6. During .this process, the temperature of the injected water comes finally, at the point where it runs off below, nearly up to that of the gas entering at this place, while,.on the other hand, the gas leaves the top partiof the cooler A at cl with a temperature slightly above that of the injected water. The strong cooling of .the gases causes all condensable constituents of itthat .is to say, the tar including the naphthalene and besides the Water first carried along with the crude gases as steam-to separate out.

Besides, by this process, especially the elimination of tar particles is considerably furthered owing to the washing, effectof the directly injected water. The products of condensation flow along with the injected and strongly heated water through the pipe 12 into the tank E. Here,- the heavier tar, separates from the lighter water, the tar settling down at the bottom, the Water floating on top of the tar. The water flows hence, by an inclined pipe w, tothe distribution nozzles .71: on top of the heater B which serves the direct reheating of the gas while the tar can be taken out from the ;tank E bythe pipe The gas leaving thecooler A at (Z and further driven by the action of the exhauster G throughthc pipe 7, is brought first to the intermediate cooler C. the importance of which will be described later on, and hence through the pipes g and h to the heater l3 serving the direct reheating of the gas. In this heater B, the water running off from thecooler-A through pipe u is brought into intimate contact with the gas entering at the bottom at it, in exactly the same manner as in the cooler A. The temperature of the gas previously cooled is raised nearly up to that of the injected hot water and, at the same time,

of the ammonia. I The'water used in the.

)5 heater B for heating the gases flows below at 'Z into a pot t and hence intothe tank F. From thence it'is again brought, by the pump H, to the distribution nozzles 0 on top of the cooler A in-oifder to be used again for 29 thecoolingof the' hot crude gases auditor s the further treatment in the manner hereinbet'ore described.

The intermediate cooler .0 between the cooler A and the heater B is the'most importantpart of the whole installation, as only this cooler enables the maintenance and a regulation of the working of the whole plant. There are two objects mainly which will be attained by'the arrangement of the 30 said cooler C z-Firstly, by means of it, the final temperature of the gas to be cooled will be brought, on account of the additional cooling eflec ted, to a certain degree required which can be exactly controlled; secondly, in consequence of its insertion between the two se arated stages of'the process, i. e. the stage 0 the direct cooling of the gas in the cooler A on the one hand and the stage of the re,- heating of the-same in the heater B on the 'other hand, a certain decrease in tempera ture is imparted to the gas while flowing from the former to the later sta e whereby the result is attained that the heat to be transferred'passes on always at first, in the coolerA, in the direction from the gas to the circulating water and subsequently, in the heater B, in the reversed way from the water to the gas. I

The arrangement of the additional cooling effected by the intermediate coolerC after the main-cooling which takes place in.

the direct cooler A is of considerable value in view of the fact that the final teinp'era-.

ture of the cooled gas obtained in the direct coolerA will be independently regulated by itself, as soon as a permanent state has been reached, to an equilibrium the degree of which will vary as the conditions of working I in the plant are altered, especially as the temperature of the crude gas entering the process will be higher or lower. By the are rangement of the special intermediate cooler C which is worked separately foritself, means are given to secure always, by the aid of a suitable additional cooling, a final tem- ,perature 01' the cooled gas which for the I whole process and especially for an'efl'ective separation of the tar, is the most favorable.

The requirement of inserting a special decrease in temperature of the gas between the two stages of the direct cooling inthe cooler A andfthe direct reheating in the heater plant which has to serve in turn, over andtwo pointsrespe'ctiveiy, so that the transi- H tion of heat takes place in both cases as'deover again, for the' cooling and reheating. of the gas.

It is a peculiarity of the ,method hereinbefore described that the water used in 0on tinuous circulation has, upon leaving the heater B wherein it has served the heating of the gas, the same temperature as it has I .upon entering immediately afterward the cooler A (at the top part at 0), wherein it serves now the cooling of the gases. Now,

by arranging the intermediate Cooler 0 and thereby causing a decrease in temperature of the gas conducted through the same,'-it' results that the temperature of the gas upon leaving the cooler A is somewhat above,

and upon entering the heater B is somewhat below the temperatureof the Water, at these sired.

The cooler itself can be made as acooler of the tubular type and worked bymeans of cooling water in an indirect way; this water which is taken from any separate source can be supplied, for instance, through the inlet m below into the space surrounding'the tubes and discharged through the upper outlet The small quantities of water condensed from the gas during this cooling can be r covered separatelyand let ofl at 0 into the pot w. From thence. the c oridensed water fiows to the storage tank F; into the cooling '1' I waterstored therein. The gab, afterhaving J left the saturater D in which, all ammonia is recovered as a solid salt, .is then conducted through thepipe nto thet'final cooler K, in order to be cooled down to such a temper atu're as is suitable. for and required .by its 'furtheruse. 'The cooler is here also shown as anindirectly acting cooler of the tubular type, which is worked by means-of cooling water in asimilar way as the. intermediate cooler- C described above, so that the condensing water whichis eliminated-withseparately,'and will be let out into the pot o.

This'oon'densing water separated out is a,

very pure water and containsno admixture whatsoever. Therefore, the final cooler K can also be formed as a directly working cooler, bringing the gas in direct contact '120 v in it from the. gas can be recovered again v K and connected to the suction pipe 9 of beginning. The greater quantity of heat K, together with the main flow of gas to the greater volume, its faculty of absorb-.

hydraulic main on top of the coke ovens, or

main, by the heatof the highly heated crude ins-sees injected cooling water. The cooled gas leaves the cooler K through the connection 2' and thence it is conducted to the places of its further use.

tin improved and far" easier manner of performing the whole process can be "attained by reconducting a part of the completely treated gas, which has left the cooler through the heater B. This is carried; out in the following way ':--A pipe r is branched oii from the connection p of the cooler the exhauster G, a damper or valve 3 being provided. By this means, the volume of the cooled gas to be carried through the heater B can be increased by any required volume of gas which has likewise been cooled. The result is that the gas passing through the heater B increases, according ing steam, and this guarantees that the water which was condensed during the first cooling of the gas in the cooler A is again completely absorbed by the gas in form of steam in the heater B during the subsequent reheating. n v

Another improvement and perfection of theprocess is attained by taking off continuously a quantity of the water collected in the tank E and conducting it into the the retorts from which the gases to be treated are originally obtained. Inside of this gas, the water brought-in is turned into steam and carried in this state, along with the gas, into the cooler A at a. The result is that the quantityof heat contained in the gas which enters at a is considerably increased by the addition oi the heat of the steam without necessitating a higher temperature of the gas. It appears that in this way an advantageous use is made of the heat contained in the highly heated crude gas in the hydraulic main on top of the ovens, which, otherwise, would be lost on account of the cooling effect of the s'urrounding atmosphere. By increasing the heat of the gas to be treated, there is the advantage that thereby a greater amount of heat is introduced into the process from the is, of course, later on to be found in the water serving the direct cooling and reheating respectively and facilitates correspondingly the reheating of the gases in the heater B.

The stream of water continuously circulating between the cooler A and the heater B absorbs, as a matter of fact, a certain quantity of free ammonia (NIL) on some places, but then, on other places of the circulation, the lure quantity of ammonia must i be rendered to the gas by the action of the 1 heat, because only a certain quantity of water is used over and over again, which, as a whole, can absorb only a certain and hm- "ited quantity of free ammonia. It is thereby insured, that, after obtaining a perma nent state in the whole system, the whole of the free ammonia originally contained in the crude gas is immediately carried to the saturater D wherein it is recovered directly as a solid ammonia salt. In the case however that the crude gas contains ammonia also in fixed form, the ammonia will go over to the water serving for direct cooling and reheating respectively, but it :does not return to the gas, because the mere influence of heat is not suiiicient to free the fixed ammonia. The water used in circulation must, therefore, gradually be enriched with ammonia salts. In this case it is advisable to let the Water be enriched to a certain concentration with fixed ammonia and then to draw off regularly certain quantities, the deficiency being made up, if necessary, with the addition of fresh water. The ammonlacal salt lye removed can either be added directly to the saturater D, presumed that this does not prove to be too strong a dilution of the saturation bath, or, any agreeable method may be employed to free the ammonia'from the liquor and to render it accessible for saturation. The most simpleway towork up the ammoniacal salt lye isto distil it in the usual way by adding lime and to conduct the ammonia vapors, which arise from this treatment, together with the gas leaving the heater B, into the saturater D.

The advantages of the process consistin the success obtained as regards the separati'on of tar and the extraction of ammonia. As regards to the separation of tar, the first advantage is to separate the tar by an intensive cooling of the gas. In comparison with the process of washing out the tar from the hot crude gases, a complete removal of the tar constituents and especially of the naphthalene is obtained by the means described.

tion of ammonia is that the gases being completely free of tar can be saturated with the whole quantity of free ammonia contained in I the crude gases. This success is arrived at without specially treating any large quantities of condensed water for the abstraction of ammonia. Contrasted with the usual process, 2'. 0., firstly to cool the gas in tubular coolers and then to saturate the cooled gas with acid for extracting ammonia, which prov involves very extensive arrangetor treating the great quantities of condensed in the cooling of the gas,

10 rate recovery'of-the by-products, tar and,

' .venient manner is attained monia are absolutely impossible because all the fixed ammonia goes over to the Water. used for direct cooling and reheating respectively, and can be obtained again without loss from it. v a The process enables the complete and sepaammonia from the coal gas in a way,-which, ontheone hand, is quite simple and convenient, on the other hand, free from all difliculties and troubles; covery ofthese by-products in the most conand assured. 'What I claim is a 1. The process for recovering tar and ammonia from'coalgas, which consists in-co0l ing the hot crude gas by water brought directly in contact therewith for separating out the tar'and, after a special intermediate cooling of the gas, reheatingtheilatter by water used previously for direct coo-ling of the 5 gas, the Water itself being used in circulation alternately for cooling and reheating the gas, then conducting the reheated gas through a saturationbath for absorbing theammonia, and finally cooling the gas free from tar and-ammonia to the temperature necessary for further use, substantially as specified. p

2. The process-for recovering tar and ammonia from coal gas, which consists in cooling the hot crude gas by water brought directly in contact therewith for separating out the tar and, after a special intermediate Thereby, Y the recooling of the gas, reheating the latter by water used previously for direct cooling of the gas, thewater itself being used in circulation alternately for cooling and reheating the gas, then conducting the reheated through a saturation'bath forabsorbing the ammonia, finally cooling the gas free from tar and ammonia to the temperature necessary for further use, and reconducting continuously a certain volume of the finally cooled gas to the main flow of gas t'o'be led into the direct heater and afterward into the saturation bath, substantially as specified.

3. The process .for' recovering tarand ammonia from coalgas, which consists incooling' the hot crude gas by water brought directly in contact therewith for separating outthe tar and, after a special intermediate cooling of the gas, reheating the'latter byv waterused previously for directcooling of the gas, the Water itself being used in circulation alternately for cooling and reheating the gas and a part of the water being continuously; taken, off and conducted into the hydraulic main of the ovens from which the gas is originally obtained, then conducting the re heated gas through a saturation bath for-absorbing the ammonia, and finally cooling the gas free from tar and ammonia to the temperature necessary for further use, substantially as specified.

In testimony whereof I have afiixed my signature in presence of two witnesses;

CARL STILL.

Witnesses:

ARTHUR KUHN, GUSTAV LAMBERTZ. 

